Ethanolamine → HCID 178433882, compound

HRID 59621Notes

Reaction equation

HRID 59621 reaction equation
[CH3:1][C:2]1[CH:3]=[C:4]([N:9]2[C:13](=[O:14])[C:12](=[N:15][NH:16][C:17]3[C:18]([OH:32])=[C:19]([C:23]4[CH:28]=[CH:27][CH:26]=[C:25]([C:29]([OH:31])=[O:30])[CH:24]=4)[CH:20]=[CH:21][CH:22]=3)[C:11]([CH3:33])=[N:10]2)[CH:5]=[CH:6][C:7]=1[CH3:8].[CH2:34]([CH2:36][NH2:37])[OH:35]>O>[CH3:8][C:7]1[CH:6]=[CH:5][C:4]([N:9]2[N:10]=[C:11]([CH3:33])/[C:12](=[N:15]/[NH:16][C:17]3[CH:22]=[CH:21][CH:20]=[C:19]([C:23]4[CH:28]=[CH:27][CH:26]=[C:25]([C:29]([OH:31])=[O:30])[CH:24]=4)[C:18]=3[OH:32])/[C:13]2=[O:14])=[CH:3][C:2]=1[CH3:1].[CH2:36]([NH2:37])[CH2:34][OH:35]

Participants

4

Reactant 2

HCID 700EthanolamineHCID 178433881HCID 178433881, compound

Product 1

HCID 178433882HCID 178433882, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

To a mixture of 3′-{N′-[1-(3,4-dimethylphenyl)-3-methyl-5-oxo-1,5-dihydro-pyrazol-4-ylidene]hydrazino}-2′-hydroxybiphenyl-3-carboxylic acid (2 g) in water (40 mL), ethanolamine (2.5 g) was added and heated to about reflux temperature for about 2 hours. The mixture was cooled to about 0° C. to about 10° C. and stirred for about 1 hour. The reaction mixture was filtered, washed with water (10 mL) and dried in an oven at about 55° C. to about 60° C. for about 12 hours to get purple solid.

Workup

  1. additionwas added
  2. temperatureheated
  3. temperatureto about reflux temperature for about 2 hours
  4. temperatureThe mixture was cooled to about 0° C. to about 10° C.
  5. filtrationThe reaction mixture was filtered
  6. washwashed with water (10 mL)
  7. customdried in an oven at about 55° C. to about 60° C. for about 12 hours
  8. customto get purple solid

Sources & evidence

ORD record
ord-701f055508c44c7799bed306935e5604
Source dataset
uspto-grants-2016_09
Patent number
US09440927B2

Reaction notes

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